CN113371738A - Preparation method for preparing lithium carbonate and co-producing magnesium hydroxide nanosheet by using feed liquid containing lithium and magnesium - Google Patents
Preparation method for preparing lithium carbonate and co-producing magnesium hydroxide nanosheet by using feed liquid containing lithium and magnesium Download PDFInfo
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- CN113371738A CN113371738A CN202010115333.4A CN202010115333A CN113371738A CN 113371738 A CN113371738 A CN 113371738A CN 202010115333 A CN202010115333 A CN 202010115333A CN 113371738 A CN113371738 A CN 113371738A
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 109
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 239000007788 liquid Substances 0.000 title claims abstract description 106
- 239000011777 magnesium Substances 0.000 title claims abstract description 82
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 80
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 title claims abstract description 42
- 239000000347 magnesium hydroxide Substances 0.000 title claims abstract description 42
- 229910001862 magnesium hydroxide Inorganic materials 0.000 title claims abstract description 42
- 239000002135 nanosheet Substances 0.000 title claims abstract description 31
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 title claims abstract description 24
- 229910052808 lithium carbonate Inorganic materials 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000000926 separation method Methods 0.000 claims abstract description 27
- 239000002002 slurry Substances 0.000 claims abstract description 27
- 238000001035 drying Methods 0.000 claims abstract description 26
- 238000005406 washing Methods 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000001556 precipitation Methods 0.000 claims abstract description 17
- 239000000047 product Substances 0.000 claims abstract description 17
- 239000007787 solid Substances 0.000 claims abstract description 16
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 15
- 239000002244 precipitate Substances 0.000 claims abstract description 10
- 239000011550 stock solution Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 57
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims description 16
- 229910001425 magnesium ion Inorganic materials 0.000 claims description 15
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 14
- 239000001099 ammonium carbonate Substances 0.000 claims description 14
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 13
- 239000003513 alkali Substances 0.000 claims description 13
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 13
- 229910001416 lithium ion Inorganic materials 0.000 claims description 13
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 12
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Substances [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 11
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 10
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 9
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 8
- 150000001768 cations Chemical class 0.000 claims description 7
- 239000012527 feed solution Substances 0.000 claims description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 7
- 235000017550 sodium carbonate Nutrition 0.000 claims description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 239000004202 carbamide Substances 0.000 claims description 6
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 6
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 6
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 6
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 5
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 5
- 235000011181 potassium carbonates Nutrition 0.000 claims description 5
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 4
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 4
- 239000011736 potassium bicarbonate Substances 0.000 claims description 4
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 4
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 4
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims description 2
- 150000001450 anions Chemical class 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 235000013877 carbamide Nutrition 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims 1
- 238000007670 refining Methods 0.000 abstract description 6
- 238000012958 reprocessing Methods 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 description 9
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000005342 ion exchange Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- 239000012267 brine Substances 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 229910001424 calcium ion Inorganic materials 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- GCICAPWZNUIIDV-UHFFFAOYSA-N lithium magnesium Chemical compound [Li].[Mg] GCICAPWZNUIIDV-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Inorganic materials [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
- C01F5/20—Magnesium hydroxide by precipitation from solutions of magnesium salts with ammonia
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
- C01F5/22—Magnesium hydroxide from magnesium compounds with alkali hydroxides or alkaline- earth oxides or hydroxides
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/22—Particle morphology extending in two dimensions, e.g. plate-like with a polygonal circumferential shape
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- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
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- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a preparation method for preparing lithium carbonate and co-producing magnesium hydroxide nanosheets from lithium and magnesium-containing feed liquid, which comprises the following steps: 1, adjusting the pH value of a lithium-containing and magnesium-containing stock solution, and reacting for 0.5-24 hours at a reaction temperature to obtain magnesium precipitate slurry; 2, carrying out solid-liquid separation on the magnesium precipitation slurry obtained after the step 1 is finished, washing and drying a solid part to obtain a magnesium hydroxide nanosheet, and obtaining a lithium-containing feed liquid with magnesium removed from a liquid part; 3, adding carbonate into the lithium-containing feed liquid without magnesium obtained in the step 2, and reacting for 0.1-12 hours to obtain lithium precipitate slurry; and 4, carrying out solid-liquid separation, washing and drying on the lithium precipitation slurry obtained in the step 3 to obtain a lithium carbonate product. The method realizes the refining magnesium removal in the lithium-containing feed liquid and the preparation of the high-valued magnesium hydroxide nanosheet in one step, and the obtained magnesium hydroxide nanosheet is regular in shape, less in lithium entrainment, free from reprocessing and capable of being directly used in practical applications such as flame retardance and the like.
Description
Technical Field
The invention belongs to the technical field of inorganic chemistry, and particularly relates to a preparation method for preparing lithium carbonate and co-producing magnesium hydroxide nanosheets from feed liquid containing lithium and magnesium.
Background
The Qinghai is rich in salt lake resources, wherein the salt lake resources are rich in magnesium, lithium, potassium, sodium and other resources. Wherein, the physical and chemical properties of the magnesium and the lithium are similar, and the separation difficulty is large. The current method for extracting lithium from salt lake mainly comprises the following steps: (1) precipitation, (2) adsorption, (3) calcination, (4) membrane separation, and (5) extraction. The method such as adsorption method, calcination method, membrane separation method and the like has the advantage of well reducing the magnesium-lithium ratio, and is particularly suitable for extracting lithium from salt lakes such as Qinghai, Tibet, Vivian and the like. However, in the purification solution in which the magnesium-lithium ratio is reduced by these methods, a part of magnesium still exists, and the existence of this part of magnesium affects the quality of lithium salts such as lithium carbonate, lithium hydroxide, and lithium chloride, and therefore, it is necessary to purify magnesium in the lithium-containing purification solution.
The traditional method for refining and removing impurities from lithium-containing feed liquid comprises an ion exchange method and a chemical precipitation method. The ion exchange method is to make the feed liquid pass through an ion exchange column capable of removing magnesium to remove the magnesium in the feed liquid, and is suitable for the feed liquid with extremely low magnesium content. The precipitation method is a widely used method, and generally, an alkali solution is added into a lithium-containing feed liquid at a certain temperature, magnesium ions are converted into magnesium hydroxide, and the magnesium hydroxide is precipitated, filtered and removed. Magnesium hydroxide nanosheets have led extensive research by scholars because they exhibit more excellent effects in flame retardancy.
The prior art for preparing magnesium hydroxide or magnesium hydroxide nanosheets mainly has the following defects:
1. a multi-step operation such as a hydrothermal modification method, a seed crystal method, a conversion method, etc. is required.
2. A morphology directing agent such as an organic base, a seed, or a surfactant is required in the direct precipitation method (as described in patent document CN 106673027A). Not only increases the cost of raw materials, but also causes impure products.
3. The existing method for removing magnesium mainly comprises an adsorption method and a precipitation method, and magnesium hydroxide obtained by the precipitation method usually has high impurity content and irregular shape, so that the magnesium hydroxide is abandoned by enterprises. Or further modification and impurity removal are needed for utilization. The by-product contains a large amount of lithium, magnesium and other resources, and is wasted when being abandoned. Further modification or removal of impurities increases the process and production costs.
Disclosure of Invention
The invention provides a preparation method for preparing lithium carbonate and co-producing magnesium hydroxide nanosheets from lithium and magnesium-containing feed liquid, the method realizes refining magnesium removal in the lithium-containing feed liquid and preparation of high-valued magnesium hydroxide nanosheets in one step, and the obtained magnesium hydroxide nanosheets are regular in shape, less in lithium entrainment, free of reprocessing, and capable of being directly used in practical applications such as flame retardance and the like.
A preparation method for preparing lithium carbonate and co-producing magnesium hydroxide nanosheets from feed liquid containing lithium and magnesium comprises the following steps:
step 1, adjusting the pH value of a lithium-containing and magnesium-containing stock solution to 7.2-13.5, and reacting at the reaction temperature of 40-180 ℃ for 0.5-24 h to obtain magnesium precipitate slurry;
step 2, carrying out solid-liquid separation on the magnesium precipitation slurry obtained after the step 1 is finished, washing and drying a solid part to obtain a magnesium hydroxide nanosheet, and obtaining a lithium-containing feed liquid with magnesium removed from a liquid part;
step 3, adding carbonate into the lithium-containing feed liquid without magnesium obtained in the step 2, wherein the molar weight of the carbonate is 0.55-2.0 times of that of lithium in the lithium-containing feed liquid without magnesium, and reacting for 0.1-12 hours at 50-150 ℃ to obtain lithium precipitate slurry, wherein the carbonate is at least one of sodium carbonate, potassium carbonate, ammonium bicarbonate, sodium bicarbonate and potassium bicarbonate;
step 4, carrying out solid-liquid separation, washing and drying on the lithium precipitation slurry obtained in the step 3 to obtain a lithium carbonate product; the solid-liquid separation, washing and drying processes are all carried out at 50-150 ℃;
the content of magnesium ions in the feed liquid containing lithium and magnesium is 0.01-200 g/L, and the content of lithium ions is 0.01-50 g/L.
In the technical scheme, the process of adjusting the pH value of the lithium and magnesium-containing material liquid to 7.2-13.5 is realized by adding an alkali solution into the pre-precipitation material liquid, wherein the alkali solution is one or more of a NaOH solution, a KOH solution, a LiOH solution, an ammonia water solution, a hydrazine hydrate solution, an ammonium bicarbonate solution, a sodium bicarbonate solution, an ammonium bicarbonate solution, a hexamethylenetetramine solution or a urea solution.
In the technical scheme, the concentration of the alkali solution is 0.1-8 mol/L.
In the technical scheme, the content of magnesium in the lithium and magnesium-containing feed liquid is 0.1-60 g/L, and the content of lithium is 0.1-40 g/L.
In the technical scheme, the magnesium hydroxide nanosheet is 10-500 nm in particle size, 5-50 nm in thickness, and is of a sheet structure, and further is of a hexagonal sheet structure.
In the technical scheme, the reaction temperature in the step 1 is 80-150 ℃.
A method for refining a feed liquid containing lithium and magnesium, removing magnesium and producing magnesium hydroxide nanosheets in parallel comprises the following steps:
step 1, adding a co-additive into a feed liquid containing lithium and magnesium, uniformly dispersing to obtain a pretreated feed liquid, adjusting the pH of the pretreated feed liquid to 7.2-13.5, and reacting at a reaction temperature of 90-130 ℃ for 0.5-24 h to obtain magnesium precipitate slurry;
the assistant is inorganic salt, the cation in the inorganic salt is at least one cation in Li, K, Na, Ca, Zn, Ni, Co or Cu, and the anion in the inorganic salt is at least one of chloride, bromide, nitrate, sulfate, borate or carbonate;
the molar ratio of the sum of the molar weight of the co-assistant cations to the magnesium ions in the pretreated feed liquid is (0.1-10): 1;
step 2, carrying out solid-liquid separation on the magnesium precipitation slurry obtained after the step 1 is finished, washing and drying a solid part to obtain a magnesium hydroxide nanosheet, and obtaining a lithium-containing feed liquid with magnesium removed from a liquid part;
step 3, adding carbonate into the lithium-containing feed liquid with magnesium removed obtained in the step 3, wherein the molar weight of the carbonate is 0.55-2.0 times of that of lithium in the lithium-containing feed liquid with magnesium removed, and reacting for 0.1-12 hours at 50-150 ℃ to obtain lithium precipitate slurry, wherein the carbonate is at least one of sodium carbonate, potassium carbonate, ammonium bicarbonate, sodium bicarbonate, potassium bicarbonate or urea;
step 4, carrying out solid-liquid separation, washing and drying on the lithium precipitation slurry obtained in the step 3 to obtain a lithium carbonate product; the solid-liquid separation, washing and drying processes are all carried out at 50-150 ℃;
the content of magnesium ions in the feed liquid containing lithium and magnesium is 0.5-30 g/L, the content of lithium ions is 0.5-30 g/L, and the sum of the molar weight of cations of the auxiliary agent is higher than 0.5 time of the molar weight of magnesium ions;
the process of adjusting the pH value of the lithium and magnesium-containing feed liquid to 7.2-13.5 is realized by adding an alkali solution into the lithium and magnesium-containing feed liquid, wherein the alkali solution is one or more of a NaOH solution, a KOH solution, a LiOH solution, an ammonia water solution, a hydrazine hydrate solution, an ammonium bicarbonate solution, a sodium bicarbonate solution, an ammonium bicarbonate solution, a hexamethylenetetramine solution or a urea solution, and the concentration of the alkali solution is 0.5-5 mol/L.
The invention has the advantages and beneficial effects that:
the method realizes the refining magnesium removal in the lithium and magnesium-containing feed liquid and the preparation of high-value magnesium hydroxide nanosheets in one step, and the obtained magnesium hydroxide nanosheets have regular shapes, less lithium entrainment and no need of reprocessing, and can be directly used in practical applications such as flame retardance and the like. The prepared lithium carbonate has high purity.
Drawings
FIG. 1 is a scanning electron micrograph of a magnesium hydroxide product obtained in example 1;
FIG. 2 is a scanning electron micrograph of the magnesium hydroxide product obtained in example 2.
For a person skilled in the art, other relevant figures can be obtained from the above figures without inventive effort.
Detailed Description
In order to make the technical solution of the present invention better understood, the technical solution of the present invention is further described below with reference to specific examples.
Example one
A method for refining a feed liquid containing lithium and magnesium, removing magnesium and producing magnesium hydroxide nanosheets in parallel comprises the following steps:
7L of feed liquid containing lithium and magnesium, wherein Mg is contained in the feed liquid containing lithium and magnesium2+Content 1g/L, Li+The content is 15 g/L; sodium hydroxide with a concentration of 1mol/L was added dropwise to the feed solution at a rate of 2ml/s with a stirring speed of 500rpm until pH 10 gave a slurry, which was then subjected to reaction crystallization at 120 ℃ for 12 hours. Then carrying out solid-liquid separation, washing and drying the solid part to obtain a magnesium hydroxide nanosheet, obtaining a magnesium-removed lithium-containing feed liquid from the liquid part, wherein the content of lithium in the separated magnesium-removed lithium-containing feed liquid is 13g/L, and the content of magnesium is 0.05 g/L; adding 1200g of sodium carbonate into the lithium-containing feed liquid with magnesium removed at 80 ℃ for reaction for 2 hours, then carrying out hot filtration at 80 ℃, and filtering to obtain solidWashing the lithium carbonate body by deionized water at the temperature of 80 ℃, and drying to obtain a lithium carbonate product. FIG. 1 is a scanning electron micrograph of the magnesium hydroxide obtained in example 1, wherein it can be seen that the magnesium hydroxide has a regular hexagonal plate-like structure with a diameter of 40nm to 130 nm. The content of magnesium ions in the lithium carbonate product after separation and washing is lower than 0.5 ppm.
Example two
1000ml of lithium-containing feed liquid is prepared, wherein Mg2+Content of 100g/L, Ca2+Content 0.1g/L, Li+With a content of 5g/L (molar ratio of lithium to magnesium of 0.17), KNO was added thereto at a stirring speed of 250rpm3The concentration was adjusted to 20g/L, and sodium hydroxide was added dropwise to the feed solution at a concentration of 2.5mol/L until the pH was 11, followed by reaction at 90 ℃ for 24 hours. And then carrying out solid-liquid separation, washing and drying the solid part to obtain a magnesium hydroxide nanosheet, obtaining a magnesium-removed lithium-containing feed liquid from the liquid part, adding sodium carbonate with the molar mass being 2 times of that of lithium ions in the lithium-containing feed liquid at 80 ℃ into the separated magnesium-removed lithium-containing feed liquid for reacting for 2 hours, carrying out heat filtration at 80 ℃, washing the filtered solid by hot water at 80 ℃, and drying to obtain a lithium carbonate product, wherein the lithium content in the separated magnesium-removed lithium-containing feed liquid is 4.95g/L, and the magnesium content in the separated magnesium-removed lithium-containing feed liquid is 0.1 g/L. FIG. 2 is a scanning electron micrograph of a magnesium hydroxide product obtained in example two, wherein the magnesium hydroxide has a hexagonal plate-like structure with a particle size of 40-80 nm. The content of magnesium ions in the obtained lithium carbonate product is lower than 1ppm, and the concentration of calcium ions is lower than 20 ppm.
EXAMPLE III
200ml of lithium-containing feed liquid is prepared, wherein Mg2+Content 1g/L, Li+The content was 15g/L (molar ratio of lithium and magnesium 51.67), LiCl was added to give a concentration of 0.2g/L, and aqueous ammonia having a concentration of 0.5mol/L was added dropwise to the feed at a rate of 1ml/s at 400rpm until the pH became 7.2 to give a slurry, which was then crystallized at 100 ℃ for 16 hours. Then carrying out solid-liquid separation, washing and drying the solid part to obtain magnesium hydroxide nanosheets, obtaining a magnesium-removed lithium-containing feed liquid from the liquid part, wherein the content of lithium in the separated magnesium-removed lithium-containing feed liquid is 15.18g/l, the content of magnesium is 0.05g/l, and the content of lithium in the magnesium-removed lithium-containing feed liquid is 80 g/lAdding potassium carbonate with the molar mass 0.55 time of lithium ions in the lithium-containing feed liquid into the mixture to react for 2 hours, then carrying out hot filtration at the temperature of 80 ℃, washing the solid obtained by filtration by hot deionized water at the temperature of 80 ℃, and drying to obtain a lithium carbonate product.
Example four
Collecting lithium-containing brine 5000ml, wherein Mg2+The content is 15g/L (0.63mol/L), KCl is 3g/L, LiCl is 20g/L, NaNO3Is 22g/L, Li2SO45g/L, (total of all auxiliaries 0.805mol/L) potassium hydroxide in a concentration of 0.5mol/L was added dropwise to the lithium-containing brine until the pH was 10 and reacted at 120 ℃ for 12 h. After the reaction is finished, carrying out solid-liquid separation, washing and drying the solid part to obtain the magnesium hydroxide nanosheet, wherein the LiCl content in the liquid phase after the solid-liquid separation is 20g/l, and the Mg content is2+Is 0.2 g/L. And adding ammonium carbonate with the molar mass 1.5 times that of lithium ions in the lithium-containing feed liquid into the magnesium-removed lithium-containing feed liquid at 80 ℃ to react for 2 hours, then carrying out hot filtration at 80 ℃, washing the solid obtained by filtration with deionized water at 80 ℃, and drying to obtain a lithium carbonate product.
EXAMPLE five
2000ml of lithium-containing feed liquid, wherein Mg2+Content of 10g/L, Li+The content of the solution was 15g/L (molar ratio of lithium to magnesium: 5.17), ZnCl was added2The concentration was adjusted to 0.2g/L, hydrazine hydrate at a concentration of 1.5mol/L was added dropwise to the feed solution at a rate of 1ml/s at a rotation speed of 400rpm until the pH became 9.5 to obtain a slurry, and the slurry was then subjected to crystallization reaction at 160 ℃ for 10 hours. And after the reaction is finished, performing solid-liquid separation on the slurry, washing and drying the solid part to obtain magnesium hydroxide nanosheets, wherein the content of lithium in the liquid phase after the solid-liquid separation is 14.9g/L and the content of magnesium is 0.01g/L, adding ammonium bicarbonate with the molar mass being 2.0 times of that of lithium ions in the lithium-containing feed liquid into the magnesium-removed lithium-containing feed liquid at 80 ℃ for reaction for 2 hours, performing heat filtration at 80 ℃, washing the filtered solid by deionized water at 80 ℃, and drying to obtain a lithium carbonate product.
EXAMPLE six
500ml of lithium-containing feed solution, wherein Mg2+The content was 12g/L, the Li + content was 5g/L (molar ratio of lithium to magnesium was 1.43), Co (NO) was added3)2Make it to be concentrated0.5g/l, 1mol/l sodium hydroxide was added dropwise to the feed solution at a rate of 1ml/s at a rotation speed of 350rpm until the pH became 10 to give a slurry, which was then crystallized at 130 ℃ for 16 hours. And after the reaction is finished, performing solid-liquid separation on the slurry, washing and drying the solid part to obtain magnesium hydroxide nanosheets, wherein the lithium content in the liquid phase after the solid-liquid separation is 4.88g/l, and the magnesium content is 0.05g/l, adding sodium carbonate with the molar mass 1.2 times that of lithium ions in the lithium-containing feed liquid into the magnesium-removed lithium-containing feed liquid at 80 ℃ for reaction for 2 hours, performing heat filtration at 80 ℃, washing the filtered solid with deionized water at 80 ℃, and drying to obtain a lithium carbonate product.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (8)
1. A preparation method for preparing lithium carbonate and co-producing magnesium hydroxide nanosheets from feed liquid containing lithium and magnesium is characterized by comprising the following steps:
step 1, adjusting the pH value of a lithium-containing and magnesium-containing stock solution to 7.2-13.5, and reacting at the reaction temperature of 40-180 ℃ for 0.5-24 h to obtain magnesium precipitate slurry;
step 2, carrying out solid-liquid separation on the magnesium precipitation slurry obtained after the step 1 is finished, washing and drying a solid part to obtain a magnesium hydroxide nanosheet, and obtaining a lithium-containing feed liquid with magnesium removed from a liquid part;
step 3, adding carbonate into the lithium-containing feed liquid without magnesium obtained in the step 2, wherein the molar weight of the carbonate is 0.55-2.0 times of that of lithium in the lithium-containing feed liquid without magnesium, and reacting for 0.1-12 hours at 50-150 ℃ to obtain lithium precipitate slurry, wherein the carbonate is at least one of sodium carbonate, potassium carbonate, ammonium bicarbonate, sodium bicarbonate and potassium bicarbonate;
step 4, carrying out solid-liquid separation, washing and drying on the lithium precipitation slurry obtained in the step 3 to obtain a lithium carbonate product; the solid-liquid separation, washing and drying processes are all carried out at 50-150 ℃;
the content of magnesium ions in the feed liquid containing lithium and magnesium is 0.01-200 g/L, and the content of lithium ions is 0.01-50 g/L.
2. The preparation method according to claim 1, wherein the adjusting of the pH of the lithium and magnesium-containing feed solution to 7.2-13.5 is performed by adding an alkali solution to the pre-precipitation feed solution, wherein the alkali solution is one or more of a NaOH solution, a KOH solution, a LiOH solution, an ammonia solution, a hydrazine hydrate solution, an ammonium bicarbonate solution, a sodium bicarbonate solution, an ammonium bicarbonate solution, a hexamethylenetetramine solution or a urea solution.
3. The method according to claim 2, wherein the concentration of the alkali solution is 0.1 to 8 mol/L.
4. The preparation method according to claim 1, wherein the lithium and magnesium-containing feed liquid has a magnesium content of 0.1 to 60g/L and a lithium content of 0.1 to 40 g/L.
5. The preparation method according to claim 1, wherein the magnesium hydroxide nanosheet is 10-500 nm in particle size, 5-50 nm in thickness, and has a lamellar structure.
6. The production method according to claim 5, wherein the sheet-like structure is a hexagonal sheet-like structure.
7. The method according to claim 1, wherein the reaction temperature in step 1 is 80 to 150 ℃.
8. A preparation method for preparing lithium carbonate and co-producing magnesium hydroxide nanosheets from feed liquid containing lithium and magnesium is characterized by comprising the following steps:
step 1, adding a co-additive into a feed liquid containing lithium and magnesium, uniformly dispersing to obtain a pretreated feed liquid, adjusting the pH of the pretreated feed liquid to 7.2-13.5, and reacting at a reaction temperature of 90-130 ℃ for 0.5-24 h to obtain magnesium precipitate slurry;
the assistant is inorganic salt, the cation in the inorganic salt is at least one cation in Li, K, Na, Ca, Zn, Ni, Co or Cu, and the anion in the inorganic salt is at least one of chloride, bromide, nitrate, sulfate, borate or carbonate;
the molar ratio of the sum of the molar weight of the co-assistant cations to the magnesium ions in the pretreated feed liquid is (0.1-10): 1;
step 2, carrying out solid-liquid separation on the magnesium precipitation slurry obtained after the step 1 is finished, washing and drying a solid part to obtain a magnesium hydroxide nanosheet, and obtaining a lithium-containing feed liquid with magnesium removed from a liquid part;
step 3, adding carbonate into the lithium-containing feed liquid with magnesium removed obtained in the step 3, wherein the molar weight of the carbonate is 0.55-2.0 times of that of lithium in the lithium-containing feed liquid with magnesium removed, and reacting for 0.1-12 hours at 50-150 ℃ to obtain lithium precipitate slurry, wherein the carbonate is at least one of sodium carbonate, potassium carbonate, ammonium bicarbonate, sodium bicarbonate, potassium bicarbonate or urea;
step 4, carrying out solid-liquid separation, washing and drying on the lithium precipitation slurry obtained in the step 3 to obtain a lithium carbonate product; the solid-liquid separation, washing and drying processes are all carried out at 50-150 ℃;
the content of magnesium ions in the feed liquid containing lithium and magnesium is 0.5-30 g/L, and the content of lithium ions is 0.5-30 g/L;
the process of adjusting the pH value of the lithium and magnesium-containing feed liquid to 7.2-13.5 is realized by adding an alkali solution into the lithium and magnesium-containing feed liquid, wherein the alkali solution is one or more of a NaOH solution, a KOH solution, a LiOH solution, an ammonia water solution, a hydrazine hydrate solution, an ammonium bicarbonate solution, a sodium bicarbonate solution, an ammonium bicarbonate solution, a hexamethylenetetramine solution or a urea solution, and the concentration of the alkali solution is 0.5-5 mol/L.
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